CN116904021B - Anti-skid rope leather material and preparation method thereof - Google Patents
Anti-skid rope leather material and preparation method thereof Download PDFInfo
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- CN116904021B CN116904021B CN202311160807.7A CN202311160807A CN116904021B CN 116904021 B CN116904021 B CN 116904021B CN 202311160807 A CN202311160807 A CN 202311160807A CN 116904021 B CN116904021 B CN 116904021B
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- 239000000463 material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010985 leather Substances 0.000 title claims abstract description 18
- 239000003607 modifier Substances 0.000 claims abstract description 31
- 239000004677 Nylon Substances 0.000 claims abstract description 30
- 229920001778 nylon Polymers 0.000 claims abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 28
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 229920002302 Nylon 6,6 Polymers 0.000 claims abstract description 15
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 14
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 14
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 14
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008117 stearic acid Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 57
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 52
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 33
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 22
- 229920002545 silicone oil Polymers 0.000 claims description 20
- 239000013067 intermediate product Substances 0.000 claims description 19
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- WZUUZPAYWFIBDF-UHFFFAOYSA-N 5-amino-1,2-dihydro-1,2,4-triazole-3-thione Chemical compound NC1=NNC(S)=N1 WZUUZPAYWFIBDF-UHFFFAOYSA-N 0.000 claims description 15
- QDASGLPLQWLMSJ-UHFFFAOYSA-N dichloro-ethenyl-phenylsilane Chemical compound C=C[Si](Cl)(Cl)C1=CC=CC=C1 QDASGLPLQWLMSJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000002390 rotary evaporation Methods 0.000 claims description 14
- HASCQPSFPAKVEK-UHFFFAOYSA-N dimethyl(phenyl)phosphine Chemical compound CP(C)C1=CC=CC=C1 HASCQPSFPAKVEK-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 238000010907 mechanical stirring Methods 0.000 description 12
- 230000001276 controlling effect Effects 0.000 description 9
- 239000005457 ice water Substances 0.000 description 5
- 239000001038 titanium pigment Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000007792 addition Methods 0.000 description 3
- 238000007259 addition reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 229920002160 Celluloid Polymers 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 235000010676 Ocimum basilicum Nutrition 0.000 description 1
- 240000007926 Ocimum gratissimum Species 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Abstract
The application relates to an anti-slip rope leather material and a preparation method thereof, belonging to the technical field of fire-fighting composite materials. The anti-slip rope leather material comprises the following components in parts by weight: 60-80 parts of nylon 66 salt, 25-35 parts of nylon 1010 salt, 20-30 parts of caprolactam, 14-18 parts of anti-slip modifier, 2-3 parts of stearic acid, 1.6-2.2 parts of titanium dioxide, 8.5-11 parts of magnesium hydroxide and 8-12 parts of deionized water; the silicon chain in the anti-slip modifier is used as a soft chain to be interpenetrated with nylon macromolecules, so that the rigidity of the nylon material is reduced, slight deformation can be generated to resist sliding in the friction process, the anti-slip modifier molecules are crosslinked and interlocked with the nylon molecules to provide support for the silicon chain, and the silicon chain is not easy to creep under stress, so that a stable anti-slip effect is maintained, the multi-element nitrogen-containing ring at the crosslinked chain link has a strong chelating effect, rigid metal-based particles can be enriched at the chain link to form a roughened structure, the friction coefficient of the material is improved, and the anti-slip modified nylon material has good anti-slip performance.
Description
Technical Field
The application belongs to the technical field of fire-fighting composite materials, and particularly relates to an anti-slip rope leather material and a preparation method thereof.
Background
The fire-fighting rope is a fire-fighting equipment for rescuing people, saving oneself, carrying equipment and evacuating substances in disaster sites. Fire-fighting ropes currently in use are of various types, such as twisted ropes, sandwich ropes, double-roller ropes, continuous ropes and the like, wherein the sandwich ropes have stable comprehensive performance and moderate manufacturing cost, and are widely applied.
The sandwich rope is generally composed of a rope core and a rope skin, wherein the rope core is made of steel wires or high-strength continuous fibers, the rope skin is generally made of high polymer fibers such as polyester, nylon, polyolefin and the like as a main bearing part, and the surface of the rope core is woven to play a role in protection, wherein the nylon rope skin is wear-resistant, tensile-resistant and chemical corrosion-resistant, and is widely applied to the rope skin. However, nylon materials have high rigidity and small friction with rope cores, the problem of rope skin sliding easily occurs in the practical application process, the lengths of rope skins at two ends of ropes used for a long time can greatly exceed the rope cores, the overall diameter is increased due to the fact that the rope skins are loose, connection between the ropes and pulleys is not facilitated, the ropes are knotted, and the rope strength is also reduced. Accordingly, the present application is directed to providing an anti-slip rope cover material for a fire rope.
Disclosure of Invention
In order to solve the technical problems in the background art, the application aims to provide an anti-slip rope leather material and a preparation method thereof.
The aim of the application can be achieved by the following technical scheme:
an anti-slip rope skin material comprises the following components in parts by weight:
60-80 parts of nylon 66 salt, 25-35 parts of nylon 1010 salt, 20-30 parts of caprolactam, 14-18 parts of anti-slip modifier, 2-3 parts of stearic acid, 1.6-2.2 parts of titanium dioxide, 8.5-11 parts of magnesium hydroxide and 8-12 parts of deionized water.
The anti-slip modifier is prepared by the following method:
step A1: uniformly mixing vinylphenyl dichlorosilane, triethylamine and acetone, controlling the temperature in an ice water bath to be constant at 5-15 ℃, applying 300-400rpm mechanical stirring, slowly adding hydroxyl-terminated silicone oil, controlling the adding reaction time to be 1.2-1.8h, adding methanol for mixing, performing reduced pressure rotary evaporation to remove acetone and low-boiling substances mainly comprising excessive methanol, performing rotary evaporation substrate water washing, removing water phase and performing vacuum drying to obtain an intermediate product.
Further, the hydroxyl group content of the hydroxyl-terminated silicone oil, the use amount ratio of vinylphenyl dichlorosilane, triethylamine, acetone and methanol was 0.1mol:0.1mol:10-14mL:160-240mL:50-70mL of hydroxyl-terminated silicone oil is low molecular weight silicone oil with room temperature viscosity not higher than 70mm 2 And/s, condensing vinyl phenyl dichlorosilane with hydroxyl-terminated silicone oil blocks, and terminating the end capping by using small-molecule high-activity methanol.
Step A2: uniformly mixing 3-amino-5-mercapto-1, 2, 4-triazole, dimethylphenylphosphine and dimethylacetamide under the protection of nitrogen, adding the intermediate product, stirring at high speed, dispersing, heating to 65-75 ℃, applying mechanical stirring at 100-150rpm and 300-400W/m 2 Ultraviolet irradiation, stirring at constant temperature, performing irradiation reaction for 2.5-3.5h, and repeatedly adding deionized water to remove dimethylacetamide after the reaction is finished to obtain the anti-skid modifier.
Further, the ratio of the amount of the intermediate, 3-amino-5-mercapto-1, 2, 4-triazole, dimethylphenylphosphine and dimethylacetamide was 100g:45-60mmol:80-100mg:150-220mL, 3-amino-5-mercapto-1, 2, 4-triazole is subjected to click reaction with unsaturated double bonds in the molecular structure of the intermediate product under the catalysis of ultraviolet irradiation and dimethylphenylphosphine, and 3-amino-5-mercapto-1, 2, 4-triazole is introduced onto a condensation molecular chain of the intermediate product.
A preparation method of an anti-slip rope leather material comprises the following steps:
step S1: and (3) uniformly mixing nylon 66 salt, nylon 1010 salt, caprolactam, an anti-slip modifier and deionized water, introducing nitrogen for protection, heating to 210-220 ℃, controlling the pressure to 1.5-1.7MPa, reacting for 35-45min, and then releasing the pressure to obtain the prepolymer.
Step S2: mixing the rest raw materials, adding into the prepolymerization material, mechanically stirring at 50-70rpm, reacting at constant temperature and normal pressure for 1.2-1.6h, discharging, cooling and pulverizing to obtain the anti-slip rope skin material.
Furthermore, the titanium dioxide adopts rutile titanium dioxide with fineness not lower than 5000 meshes, and mainly plays a role in shielding ultraviolet rays.
Further, the fineness of magnesium hydroxide is not lower than 2000 mesh, mainly as a flame retardant and a rigid filler.
The application has the beneficial effects that:
the anti-skid rope leather material is a nylon-based composite material, takes nylon 66 salt, nylon 1010 salt and caprolactam as base materials, and obtains good anti-skid property by introducing an independently developed anti-skid modifier; the anti-skid modifier is prepared by condensing vinyl phenyl dichlorosilane and low-molecular-weight hydroxyl-terminated silicone oil blocks, introducing chain links containing phenyl and vinyl, introducing 3-amino-5-mercapto-1, 2, 4-triazole into the chain link position through a click addition reaction, and introducing a multi-element nitrogen-containing ring and active amino; the silicon chain in the molecular chain of the anti-skid modifier is used as a soft chain and is inserted into a nylon macromolecular chain, so that the rigidity of the nylon material is reduced, slight deformation can be generated in the friction process to resist sliding, the nylon macromolecular chain provides support for the silicon chain, and the silicon chain is supported not to undergo stress creep when being subjected to friction force, so that good shape retention capability is provided for the silicon chain; the amino introduced in the chain link participates in the polymerization of nylon under high temperature and high pressure, so that a silicon chain and a nylon molecular chain form an interlocking structure, the bonding strength of the silicon chain and the nylon molecular chain is enhanced, and the stable anti-skid effect is maintained; the multi-element nitrogen-containing ring at the chain link has strong chelation effect on magnesium hydroxide and titanium pigment, can enrich the rigid metal-based particles at the chain link, forms local hardening and strengthening at the chain link, forms a roughened structure at the reinforced chain link in the friction process, improves the friction coefficient of the material, and has good anti-skid performance.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described in the following in conjunction with the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
The preparation method of the anti-slip rope leather material comprises the following specific implementation processes:
1) Preparation of anti-slip modifier
1.1 mixing vinylphenyl dichlorosilane, triethylamine and acetone, controlling temperature with ice water bath to 15 deg.C, mechanically stirring at 400rpm, slowly adding hydroxyl-terminated silicone oil (in this example, silicone oil with model X-22-170BX, and room temperature viscosity of about 40 mm) within 20min 2 And/s), continuing to stir the mixture at constant temperature after the mixture is completely added, controlling the total adding reaction time to be 1.2h, adding methanol and mixing, wherein in the reaction, the hydroxyl content of hydroxyl-terminated silicone oil, the dosage ratio of vinylphenyl dichlorosilane, triethylamine, acetone and methanol is 0.1mol:0.1mol:14mL:200mL:70mL, then removing low-boiling substances mainly comprising acetone and excessive methanol rapidly by reduced pressure rotary evaporation, mixing the rotary evaporation substrate with water, removing water phase, and drying in vacuum to obtain an intermediate product.
1.2 taking 3-amino-5-mercapto-1, 2, 4-triazole, dimethyl phenyl phosphine and dimethylacetamide, evenly mixing under the protection of nitrogen, adding intermediate products, stirring and dispersing for 5min at a high speed of 1200rpm, heating to 75 ℃, applying 150rpm mechanical stirring and 400W/m 2 Ultraviolet irradiation, stirring at constant temperature, and carrying out irradiation reaction for 2.5h, wherein in the reaction, the dosage ratio of the intermediate product, 3-amino-5-mercapto-1, 2, 4-triazole, dimethylphenylphosphine and dimethylacetamide is 100g:60mmol:100mg:220mL, adding deionized water with the mass 1.5 times of the reaction substrate for rotary evaporation after the reaction is finished, and removing the dimethylacetamide to prepare the anti-skid modifier.
2) Preparation of anti-slip rope leather material
2.1, the following raw materials are taken according to parts by weight:
80 parts of nylon 66 salt, 30 parts of nylon 1010 salt, 20 parts of caprolactam, 20 parts of industrial raw materials, 16 parts of anti-slip modifier, 2 parts of stearic acid, 1801 of stearic acid, 2.2 parts of titanium dioxide, about 5000 meshes of rutile type titanium dioxide, about 11 parts of magnesium hydroxide, about 2000 meshes of Guangdong source epitaxial powder, about 2 parts of deionized water, and about 3 parts of Guangdong Yi Beacon chemical industry Co, wherein 80 parts of nylon 66 salt is provided by Basil company, 30 parts of nylon 1010 salt is provided by Shandong celluloid company, and 16 parts of anti-slip modifier; the following examples refer to purchasing materials all using the same batch materials as described above.
2.2, adding nylon 66 salt, nylon 1010 salt, caprolactam, an anti-slip modifier and deionized water into a pressure kettle, uniformly mixing, vacuumizing, introducing nitrogen to replace air, heating to 220 ℃ in a nitrogen protection atmosphere, regulating the stop pressure of a pressure valve to 1.7MPa, performing high-temperature and constant-pressure reaction for 35min, and releasing the pressure to normal pressure after the reaction is finished to obtain the prepolymer.
2.3, premixing stearic acid, titanium pigment and magnesium hydroxide, adding into the prepolymerization material, maintaining the temperature at 220 ℃, applying 70rpm mechanical stirring, reacting for 1.2 hours at constant temperature and normal pressure, discharging, cooling after the reaction is finished, and crushing to obtain the anti-slip rope skin material.
Example 2
The preparation method of the anti-slip rope leather material comprises the following specific implementation processes:
1) Preparation of anti-slip modifier
1.1 mixing vinylphenyl dichlorosilane, triethylamine and acetone, controlling temperature with ice water bath to 5 deg.C, stirring mechanically at 300rpm, slowly adding hydroxyl-terminated silicone oil (in this example, silicone oil with model X-22-170DX, room temperature viscosity of about 65 mm) within 30min 2 And/s), continuing to stir the mixture at constant temperature after the mixture is completely added, controlling the total adding reaction time to be 1.8h, adding methanol and mixing, wherein in the reaction, the hydroxyl content of hydroxyl-terminated silicone oil, the dosage ratio of vinylphenyl dichlorosilane, triethylamine, acetone and methanol is 0.1mol:0.1mol:10mL:240mL:60mL, then decompression rotary evaporation is carried out to rapidly remove low-boiling substances mainly comprising acetone and excessive methanol, and water is used for rotary evaporation of substratesMixing, removing water phase, vacuum drying to obtain intermediate product.
1.2 taking 3-amino-5-mercapto-1, 2, 4-triazole, dimethyl phenyl phosphine and dimethylacetamide, evenly mixing under the protection of nitrogen, adding intermediate products, stirring and dispersing for 5min at a high speed of 1200rpm, heating to 65 ℃, applying mechanical stirring at 100rpm and 300W/m 2 Ultraviolet irradiation, stirring at constant temperature, and carrying out irradiation reaction for 3.5h, wherein in the reaction, the dosage ratio of the intermediate product to 3-amino-5-mercapto-1, 2, 4-triazole to dimethylphenylphosphine to dimethylacetamide is 100g:45mmol:80mg:150mL, adding deionized water with the mass 1.5 times of the reaction substrate for rotary evaporation after the reaction is finished, and removing the dimethylacetamide to prepare the anti-skid modifier.
2) Preparation of anti-slip rope leather material
2.1, the following raw materials are taken according to parts by weight:
65 parts of nylon 66 salt, 35 parts of nylon 1010 salt, 30 parts of caprolactam, 18 parts of an anti-slip modifier (prepared in the embodiment), 3 parts of stearic acid, 1.9 parts of titanium dioxide, 8.5 parts of magnesium hydroxide and 8 parts of deionized water.
2.2, adding nylon 66 salt, nylon 1010 salt, caprolactam, an anti-slip modifier and deionized water into a pressure kettle, uniformly mixing, vacuumizing, introducing nitrogen to replace air, heating to 210 ℃ in a nitrogen protection atmosphere, regulating the stop pressure of a pressure valve to 1.5MPa, reacting at a high temperature and a constant pressure for 45min, and releasing the pressure to normal pressure after the reaction is finished to obtain the prepolymer.
2.3, premixing stearic acid, titanium pigment and magnesium hydroxide, adding into the prepolymerization material, maintaining the temperature at 210 ℃, applying mechanical stirring at 50rpm, reacting for 1.6 hours at constant temperature and normal pressure, discharging, cooling after the reaction, and crushing to obtain the anti-slip rope skin material.
Example 3
The preparation method of the anti-slip rope leather material comprises the following specific implementation processes:
1) Preparation of anti-slip modifier
1.1, taking vinylphenyl dichlorosilane, triethylamine and acetone, mixing evenly, adopting an ice water bath to control the temperature to be constant at 10 ℃, applying 400rpm mechanical stirring, slowly adding hydroxyl-terminated silicone oil (X-22-170 BX) within 20min, continuing constant temperature stirring reaction after complete addition, controlling the total addition reaction time to be 1.6h, adding methanol, and mixing, wherein the ratio of the hydroxyl content of the hydroxyl-terminated silicone oil to the dosage of vinylphenyl dichlorosilane, triethylamine, acetone and methanol is 0.1mol:0.1mol:12mL:160mL: and (2) 50mL, then rapidly removing low-boiling substances mainly comprising acetone and excessive methanol by reduced pressure rotary evaporation, mixing the rotary evaporation substrate with water, removing water phase, and drying in vacuum to obtain an intermediate product.
1.2 taking 3-amino-5-mercapto-1, 2, 4-triazole, dimethyl phenyl phosphine and dimethylacetamide, evenly mixing under the protection of nitrogen, adding intermediate products, stirring and dispersing for 5min at a high speed of 1200rpm, heating to 72 ℃, applying 150rpm mechanical stirring and 340W/m 2 Ultraviolet irradiation, stirring at constant temperature, and carrying out irradiation reaction for 2.8h, wherein in the reaction, the dosage ratio of the intermediate product to 3-amino-5-mercapto-1, 2, 4-triazole to dimethylphenylphosphine to dimethylacetamide is 100g:55mmol:90mg:200mL, adding deionized water with the mass 1.5 times of the reaction substrate for rotary evaporation after the reaction is finished, and removing dimethylacetamide to prepare the anti-skid modifier.
2) Preparation of anti-slip rope leather material
2.1, the following raw materials are taken according to parts by weight:
70 parts of nylon 66 salt, 25 parts of nylon 1010 salt, 22 parts of caprolactam, 15 parts of anti-slip modifier (prepared in the embodiment), 2 parts of stearic acid, 2 parts of titanium dioxide, 9.5 parts of magnesium hydroxide and 11 parts of deionized water.
2.2, adding nylon 66 salt, nylon 1010 salt, caprolactam, an anti-slip modifier and deionized water into a pressure kettle, uniformly mixing, vacuumizing, introducing nitrogen to replace air, heating to 210 ℃ in a nitrogen protection atmosphere, regulating the stop pressure of a pressure valve to 1.6MPa, reacting at a high temperature and a constant pressure for 40min, and releasing the pressure to normal pressure after the reaction is finished to obtain the prepolymer.
2.3, premixing stearic acid, titanium pigment and magnesium hydroxide, adding into the prepolymerization material, maintaining the temperature at 210 ℃, applying 70rpm mechanical stirring, reacting for 1.4 hours at constant temperature and normal pressure, discharging, cooling after the reaction, and crushing to obtain the anti-slip rope skin material.
Example 4
The preparation method of the anti-slip rope leather material comprises the following specific implementation processes:
1) Preparation of anti-slip modifier
1.1, taking vinylphenyl dichlorosilane, triethylamine and acetone, mixing evenly, adopting ice water bath to control the temperature to be constant at 5 ℃, applying 400rpm mechanical stirring, slowly adding hydroxyl-terminated silicone oil (X-22-170 DX) within 30min, continuing constant temperature stirring reaction after complete addition, controlling the total addition reaction time to be 1.6h, adding methanol, and mixing, wherein the ratio of the hydroxyl content of the hydroxyl-terminated silicone oil to the dosage of vinylphenyl dichlorosilane, triethylamine, acetone and methanol is 0.1mol:0.1mol:12mL:220mL:60mL, then decompressing and steaming to quickly remove low-boiling substances mainly comprising acetone and excessive methanol, mixing the steaming substrate with water, removing water phase, and drying in vacuum to obtain an intermediate product.
1.2 taking 3-amino-5-mercapto-1, 2, 4-triazole, dimethyl phenyl phosphine and dimethylacetamide, evenly mixing under the protection of nitrogen, adding intermediate products, stirring and dispersing for 5min at a high speed of 1200rpm, heating to 75 ℃, applying 150rpm mechanical stirring and 300W/m 2 Ultraviolet irradiation, stirring at constant temperature, and carrying out irradiation reaction for 3.2h, wherein in the reaction, the dosage ratio of the intermediate product to 3-amino-5-mercapto-1, 2, 4-triazole to dimethylphenylphosphine to dimethylacetamide is 100g:50mmol:80mg:200mL, adding deionized water with the mass 1.5 times of the reaction substrate for rotary evaporation after the reaction is finished, and removing dimethylacetamide to prepare the anti-skid modifier.
2) Preparation of anti-slip rope leather material
2.1, the following raw materials are taken according to parts by weight:
60 parts of nylon 66 salt, 30 parts of nylon 1010 salt, 26 parts of caprolactam, 14 parts of anti-slip modifier (prepared in the embodiment), 2 parts of stearic acid, 1.6 parts of titanium dioxide, 10 parts of magnesium hydroxide and 10 parts of deionized water.
2.2, adding nylon 66 salt, nylon 1010 salt, caprolactam, an anti-slip modifier and deionized water into a pressure kettle, uniformly mixing, vacuumizing, introducing nitrogen to replace air, heating to 220 ℃ in a nitrogen protection atmosphere, regulating the stop pressure of a pressure valve to 1.6MPa, reacting at a high temperature and a constant pressure for 45min, and releasing the pressure to normal pressure after the reaction is finished to obtain the prepolymer.
2.3, premixing stearic acid, titanium pigment and magnesium hydroxide, adding into the prepolymerization material, maintaining the temperature at 220 ℃, applying 70rpm mechanical stirring, reacting for 1.4 hours at constant temperature and normal pressure, discharging, cooling after the reaction, and crushing to obtain the anti-slip rope skin material.
Comparative example
The comparative example is a commercial flame-retardant nylon master batch, which is provided by Dongguan city Star chemical Co., ltd, and the model is FR-1312.
Placing the materials obtained in examples 1-4 and comparative examples in a flat vulcanizing machine, wherein the vulcanization molding temperature of the examples is 270 ℃, the comparative examples are subjected to hot press molding according to the guide temperature of 255 ℃ and all applied with 3MPa pressure, cooling, cutting out a sample with the specification of phi 10mm, and carrying out a reciprocating friction test by adopting an HSR-2M type friction and wear tester, wherein the friction substrate is 304 stainless steel sheet, and the specific test parameters are as follows: the reciprocating frequency is 5Hz, the load is 20N, the temperature and the humidity are 65 percent, the friction data are acquired at intervals of 100 seconds, the friction coefficient is calculated, and the specific test data are shown in the table 1:
as can be seen from the data in Table 1, the friction coefficient of the test sample is increased along with the increase of the friction time, and the friction coefficient is related to the surface friction roughening of the material, and the initial friction coefficient and the friction coefficient after stabilization of the test sample are obviously higher than those of the test sample along with the progress of the friction to 2000s, so that the test sample has better anti-slip performance when applied to the rope leather material.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the application, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the application or exceeding the scope of the application as defined in the claims.
Claims (7)
1. The anti-slip rope leather material is characterized by comprising the following components in parts by weight:
60-80 parts of nylon 66 salt, 25-35 parts of nylon 1010 salt, 20-30 parts of caprolactam, 14-18 parts of anti-slip modifier, 2-3 parts of stearic acid, 1.6-2.2 parts of titanium dioxide, 8.5-11 parts of magnesium hydroxide and 8-12 parts of deionized water;
the preparation method of the anti-slip modifier comprises the following steps:
step A1: uniformly mixing vinylphenyl dichlorosilane, triethylamine and acetone, keeping the temperature at 5-15 ℃, stirring, slowly adding hydroxyl-terminated silicone oil, controlling the reaction time to be 1.2-1.8h, adding methanol for mixing, removing low-boiling substances mainly including acetone and excessive methanol by reduced pressure rotary evaporation, washing a rotary evaporation substrate, removing a water phase, and vacuum drying to obtain an intermediate product;
step A2: uniformly mixing 3-amino-5-mercapto-1, 2, 4-triazole, dimethylphenylphosphine and dimethylacetamide under the protection of nitrogen, adding an intermediate product, stirring and dispersing, heating to 65-75 ℃, stirring and applying 300-400W/m 2 Ultraviolet irradiation, stirring at constant temperature, performing irradiation reaction for 2.5-3.5h, and repeatedly adding deionized water to remove dimethylacetamide after the reaction is finished to obtain the anti-skid modifier.
2. The anti-slip rope skin material according to claim 1, wherein the hydroxyl content of hydroxyl-terminated silicone oil, the dosage ratio of vinylphenyl dichlorosilane, triethylamine, acetone and methanol is 0.1mol:0.1mol:10-14mL:160-240mL:50-70mL.
3. An anti-slip rope skin material according to claim 2Characterized in that the hydroxyl-terminated silicone oil is low molecular weight silicone oil with the room temperature viscosity not higher than 70mm 2 /s。
4. A non-slip rope cover material according to claim 3, wherein the ratio of the amount of intermediate product, 3-amino-5-mercapto-1, 2, 4-triazole, dimethylphenylphosphine and dimethylacetamide is 100g:45-60mmol:80-100mg:150-220mL.
5. The anti-slip rope cover material according to claim 1, wherein the titanium dioxide is rutile titanium dioxide with fineness not lower than 5000 meshes.
6. An anti-slip rope cover material according to claim 1, wherein the fineness of the magnesium hydroxide is not lower than 2000 mesh.
7. The method for preparing the anti-slip rope cover material according to claim 1, comprising the following steps:
step S1: mixing nylon 66 salt, nylon 1010 salt, caprolactam, an anti-slip modifier and deionized water evenly, introducing nitrogen for protection, heating to 210-220 ℃, controlling the pressure to 1.5-1.7MPa, reacting for 35-45min, and releasing pressure to obtain a prepolymer;
step S2: mixing the rest raw materials, adding into the prepolymerization material, mechanically stirring at 50-70rpm, reacting at constant temperature and normal pressure for 1.2-1.6h, discharging, cooling and pulverizing to obtain the anti-slip rope skin material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108795036A (en) * | 2018-05-24 | 2018-11-13 | 浙江心源科技有限公司 | A kind of cable cover(ing) PP Pipe Compound and cable cover(ing) based on block copolymerization nylon elastomer |
| CN108914106A (en) * | 2018-06-08 | 2018-11-30 | 浙江工业大学 | A kind of galvanized sheet surface passivation filling treatment fluid and its application certainly |
| CN111253733A (en) * | 2020-04-07 | 2020-06-09 | 长沙五犇新材料科技有限公司 | Modified nylon elastomer and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108795036A (en) * | 2018-05-24 | 2018-11-13 | 浙江心源科技有限公司 | A kind of cable cover(ing) PP Pipe Compound and cable cover(ing) based on block copolymerization nylon elastomer |
| CN108914106A (en) * | 2018-06-08 | 2018-11-30 | 浙江工业大学 | A kind of galvanized sheet surface passivation filling treatment fluid and its application certainly |
| CN111253733A (en) * | 2020-04-07 | 2020-06-09 | 长沙五犇新材料科技有限公司 | Modified nylon elastomer and preparation method and application thereof |
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